论文部分内容阅读
目的建立快速分离奥氮平及其相关物质A的胶束高效液相色谱新方法,探讨其分离机理。方法采用MicrosorbMV 100 C8色谱柱,流动相为含41.7 mmol/L的十二烷基硫酸钠、pH 2.5(用磷酸调节)的胶束溶液—乙腈(35∶65,V/V),流速1.2 mL/min,柱温为40℃。并对方法进行方法学考察,包括专属性、精密度、稳定性、线性、准确度、最低检测限、最低定量限。结果该方法专属性强(分离度>2.03,峰纯度>996),5 min内就可以测定不同片剂中奥氮平含量及其相关物质A。奥氮平标示量的百分含量为97.1%~100.4%;奥氮平相关物质A的含量为0.3%~0.6%。建立了溶质、流动相和固定相三者之间相互作用的胶束高效液相色谱模型,并基于此模型对可能的分离机理进行了详细讨论。结论该方法快速、准确、灵敏,可用于奥氮平片的质量控制。
OBJECTIVE To establish a new method for the rapid separation of olanzapine and its related substances A from micellar high performance liquid chromatography and to explore its mechanism of separation. Methods MicrosorbMV 100 C8 column was used. The mobile phase consisted of 41.7 mmol / L sodium dodecyl sulfate, pH 2.5 (35:65, V / V) / min, the column temperature is 40 ℃. Methodological study of the method, including specificity, precision, stability, linearity, accuracy, minimum detection limit, the lowest limit of quantification. Results The method is highly specific (resolution> 2.03, peak purity> 996). The content of olanzapine and its related substance A in different tablets can be determined within 5 min. The content of olanzapine labeled amount was 97.1% ~ 100.4%; the content of olanzapine related substance A was 0.3% ~ 0.6%. A micelle high performance liquid chromatography model was established for the interaction between solute, mobile phase and stationary phase, and the possible separation mechanism was discussed in detail based on this model. Conclusion The method is rapid, accurate and sensitive and can be used for the quality control of olanzapine tablets.